EP1069479B1 - Toner und Bildherstellungsverfahren - Google Patents

Toner und Bildherstellungsverfahren Download PDF

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Publication number
EP1069479B1
EP1069479B1 EP00114307A EP00114307A EP1069479B1 EP 1069479 B1 EP1069479 B1 EP 1069479B1 EP 00114307 A EP00114307 A EP 00114307A EP 00114307 A EP00114307 A EP 00114307A EP 1069479 B1 EP1069479 B1 EP 1069479B1
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Prior art keywords
toner
carbon black
image
black
magnetic
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Expired - Lifetime
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EP00114307A
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English (en)
French (fr)
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EP1069479A1 (de
Inventor
Junko Yoshikawa
Kenji Okado
Masaaki Taya
Yushi Mikuriya
Kazumi Yoshizaki
Yasushi Katsuta
Kenichi Nakayama
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Canon Inc
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Canon Inc
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/097—Plasticisers; Charge controlling agents
    • G03G9/09708—Inorganic compounds
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/0821—Developers with toner particles characterised by physical parameters
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/087—Binders for toner particles
    • G03G9/08742—Binders for toner particles comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • G03G9/08755—Polyesters
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/097—Plasticisers; Charge controlling agents
    • G03G9/09783—Organo-metallic compounds

Definitions

  • carbon black has a small primary particle diameter and a large specific surface area compared to other pigments. Therefore, carbon black is hardly dispersed or maldistributed on the surface of a toner particle and easily produces free carbon black. Because carbon black is fine powder having a high stickiness, presence of free carbon black causes the flowability of toner to deteriorate and prevents preferable frictional electrification, and particularly deteriorates the reproducibility of a half-tone image. Moreover, when carbon black is not completely dispersed, a problem also occurs that a sufficient image density is not obtained.
  • Japanese Patent Application Laid-Open No. 56-116044 discloses a method of using carbon black whose surface is grafted and Japanese Patent Application Laid-Open No. 63-210849 discloses a method of using carbon black whose surface is treated by an aluminum coupling agent.
  • it is industrially difficult to use these methods because the step of treating the surface of carbon black is complex and takes a lot of time, and requires a lot of manufacturing cost.
  • the alkali metal content in the carbon black is less than 50 ppm, dispersibility improvement of the carbon black, which is a main purpose of the present invention, can not properly be achieved.
  • the content is more than 1,000 ppm, the charging property of the carbon black is increased too much and that may inhibit polymerization especially in the case of producing a toner by the polymerization method, may increase the existence ratio of a toner bearing the opposite charge in the case of employing such a carbon black for a negative charge toner, or may cause fogging and scattering of a toner.
  • the ratio A/C wherein A (ppm) stands for the content of an alkali metal element based on the weight of a toner particle and C (% by weight) for the content of an organometallic compound is preferably 5 to 200 and more preferably 7 to 160.
  • a binder resin for the present invention not only solely a polyester resin but also together with a polyester resin, the following resins may be used.
  • the resins to be employed together with a polyester resin include, for example, styrenic copolymers such as polystyrene, styrene-butadiene copolymer, and styrene-acrylic acid copolymer; polyethylene-vinyl ethyleneacetate copolymer, phenolic resin, epoxy resin, acryl phthalate resin, polyamide resin, polyester resin, and maleic acid type resin.
  • the following production methods may be employed.
  • He gas is passed in 50 kPa pressure condition.
  • an alkane with a known number of carbons is separately injected and measurement is carried out in the same flowing out time and by comparing obtained gas chromatogram, introducing the gasified components to a weight spectrographic apparatus, or the like, the structures are identified.
  • the content ratio of ester compounds with the same number of carbons is calculated by determining the ratios of respective surface areas of respective peaks to the total surface area of all of the peaks of the obtained chromatogram.
  • the particle diameter distribution of the toner of the present invention consists of toner particles with a diameter of 4 ⁇ m or smaller preferably in 20 % by number or lower and more preferably in 5 to 15 % by number and toner particles with a diameter of 12.7 ⁇ m or larger preferably in 3.5 % by volume or lower and more preferably in 0.1 to 2.0 % by volume.
  • a loss tangent tan ⁇ can be used which is defined as the ratio of dielectric loss factor ⁇ " and dielectric constant ⁇ ' as described at page 241 of "Characteristics of Carbon Black, Optimum Mixing, and Utilization Technique" (published by Technology Information Association). The smaller the loss tangent tan ⁇ value is, the more excellent the dispersibility of the carbon black is.
  • the desirable dispersion state of a carbon black in a toner particle is that the carbon black in a binder resin exists much in the center part of the toner and less exists in the toner surface layer in the case the toner cross-section is observed by a transmission microscope.
  • fine powders of silica, alumina, and titanium oxide are mentioned.
  • the powders with a specific surface area of 30 m 2 /g or higher (more preferably 50 to 400 m 2 /g) as determined by nitrogen adsorption measured by BET method provide desirable results.
  • the addition amount of the fine powder for improving the flowability is preferably 0.01 to 8 parts by weight and more preferably 0.1 to 5 parts by weight to 100 parts by weight of toner particles.
  • a carrier comprising core particles composed of a magnetic material or a mixture of a magnetic material and a non-magnetic material and a coating of a resin and/or a silane compound formed on the core particles is preferable.
  • the carrier is mixed with a negatively chargeable toner, it is preferable to incorporate an aminosilane compound into the coating layer.
  • the volume average particle diameter of the carrier is preferably 4 to 100 ⁇ m (preferably 10 to 80 ⁇ m and more preferably 20 to 60 ⁇ m). If the volume average particle diameter of the carrier is smaller than 4 ⁇ m, together with the toner, the carrier is easily transferred to a latent image holding member in the development process and tends to cause damages on the latent image holding member and cleaning blades. On the contrary, if the volume average particle diameter of the carrier is larger than 100 ⁇ m, the toner holding capability of the carrier is deteriorated and solid image is made uneven and toner scattering and fogging or the like easily occur.
  • the measurement is carried out in accordance with DIN ISO 787/9.
  • the dielectric loss tangent (tan ⁇ ) is determined from the measured value of dielectric constants at frequencies of 5 ⁇ 10 4 Hz and 10 5 Hz.
  • Sieves with mesh sizes of 355 ⁇ m (40 meshes), 263 ⁇ m (60 meshes) and 154 ⁇ m (100 meshes) are used when the bulk density is less than 0.4 g/cm 3
  • sieves with mesh sizes of 263 ⁇ m (60 meshes), 154 ⁇ m (100 meshes) and 77 ⁇ m (200 meshes) are used when the bulk density is 0.4 g/cm 3 or more and less than 0.9 g/cm 3
  • sieves with mesh sizes of 154 ⁇ m (100 meshes), 77 ⁇ m (200 meshes) and 43 ⁇ m (325 meshes) are used when the bulk density is 0.9 g/m 3 or more.
  • Vback fogging removing voltage
  • photosensitive member By using two-component developers having satisfactorily charged toner, fogging removing voltage (Vback) can be reduced, and the primary charging of photosensitive member can be reduced, thereby making it possible to prolong the life of photosensitive member.
  • Vback depending on development systems, is preferably 350 V or less, and more preferably 300 V or less.
  • voltage for use preferably ranges from 100 V to 500 V so that adequate image density is provided.
  • developers containing the toner of the present invention due to small change in electric charge of the toner in the development device, helps to control degradation of image quality even after copying many times, together with promoting high image quality in the initial stage, and satisfactory image formation for long period is therefore achieved.
  • the adjustment blade 15 which is placed below the development sleeve 11 and adjusts the layer thickness of the developer 19 on the development sleeve 11 is a non-magnetic blade that is made from a non-magnetic material such as aluminum or SUS 316.
  • the distance between its edge and the surface of the development sleeve 11 preferably ranges from 150 ⁇ m to 1,000 ⁇ m, more preferably from 250 ⁇ m to 900 ⁇ m. If the distance is less than 150 ⁇ m, this space may be clogged with magnetic carriers to develop unevenness in the developer layer, and it is difficult to apply a developer required for performing satisfactory development and low density and uneven development images may be formed.
  • the aforesaid image forming process is repeated for yellow (Y), magenta (M), syan (C) and black (B) toner, thus obtaining a color image produced by superimposing four color toner images and transferring the same onto the recording material on the transferring drum 45.
  • the electrostatic image formed on the photosensitive member 91 is developed using these developers by development systems such as a magnetic brush development system, a non-magnetic non-component development system or a magnetic jumping development system, and a toner image of each color is formed on the photosensitive member 91.
  • the photosensitive member 91 is a conductive substrate 91b and a photosensitive drum or a photosensitive belt having a photoconductive insulating material layer 91a such as amorphous selenium, cadmium sulfide, zinc oxide, organic photoconductor and amorphous silicon formed on the conductive substrate.
  • the photosensitive member 91 is rotated in the direction of arrow by a drive unit not shown in the figure.
  • photosensitive members having an amorphous silicon photosensitive layer or an organic photosensitive layer are preferably used.
  • the non-magnetic single component developer 176 is stored in the developer container 171 and is supplied by the supply roller 173 onto the developer carrier 172.
  • the supply roller 173 which is composed of foam material such as polyurethane foam and rotates in the normal or reverse direction of the developer carrier at the relative speed other than zero, not only supplies the developer but strips off the developer on the developer carrier 172 after development (unused developer).
  • the non-magnetic single component developer supplied onto the developer carrier 172 is applied uniformly and lightly by the elastic blade 174 as a developer layer thickness control member.
  • the pressure from the elastic coating blade and the developer carrier abutting against each other ranges from 2.94 to 245 N/m (from 0.3 to 25 kg/m) as line pressure in the direction of the bus line of the development sleeve, and preferably from 4.90 to 118 N/m (from 0.5 to 12 kg/m). If the contact pressure is less than 2.94 N/m, it is difficult to apply the non-magnetic single component developer and the distribution of the amount of electrostatic charge on the non-magnetic single component developer becomes broad, thus causing fogging and scatter. If the contact pressure is more than 245 N/m, the non-magnetic single component developer receives high pressure and the developer is deteriorated, thus causing among other things the cohesiveness of the developer, which is not preferable.
  • the magnetic carrier core (A) was coated with a 5 wt.% toluene solution of ⁇ -aminopropyltrimethoxysilane, shown by the following formula: NH 2 - CH 2 CH 2 CH 2 - Si ( ⁇ OCH 3 ) 3 A shear stress was continuously applied to the magnetic carrier core (A), while it was coated, to evaporate toluene during the coating process.
  • Image density stability was evaluated by the difference between density of the image produced during the initial stage of the durability test, conducted under the H/H conditions, and that of the image on the 1000th copy.
  • Example 2 The same developer as that for Example 1, except the non-magnetic black toner 1 was replaced by the non-magnetic black toner 11 having a tan ⁇ (5 ⁇ 10 4 Hz) of 0.0115 and tan ⁇ (10 5 Hz) of 0.0102, was evaluated by the same methods.
  • the image density was higher than that observed in Example 1, but fogging, toner scattering, solid image uniformity and image density stability of the images produced under the H/H conditions were slightly inferior, as shown in Table 10, although to an extent that should cause no practical problem.
  • non-magnetic black toner 9 having a tan ⁇ (5 ⁇ 10 4 Hz) of 0.0131 and tan ⁇ (10 5 Hz) of 0.0111, was evaluated by the same methods.
  • the image density was higher than that observed in Example 1, but fogging, toner scattering, solid image uniformity and image density stability of the images produced under the H/H conditions were inferior, as shown in Table 12.
  • Example 1 The same developer as that for Example 1, except the non-magnetic black toner 1 was replaced by the non-magnetic black toner 33 containing carbon black (17) having a toluene extraction of 0.07%, was evaluated by the same methods.
  • the solid image uniformity of the images formed under the H/H conditions was slightly inferior to that observed in Example 1, as shown in Table 11, and the toner had a broad particle size distribution during the production process, although both to an extent that should cause no practical problem.
  • Example 11 The same developer as that for Example 1, except the ferrite carrier I was replaced by the ferrite carrier II, was evaluated by the same methods. The good results were produced, although the fogging was slightly increased, as shown in Table 11.
  • Example 45 The same developer as that for Example 45, except the non-magnetic black toner 43 was replaced by the non-magnetic black toner 44 containing potassium at 16 ppm, was evaluated by the same methods.
  • the image density, fogging, toner scattering solid image uniformity, and image density stability were slightly inferior to those observed in Example 45, as shown in Table 11, although to an extent that should cause no practical problem.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Inorganic Chemistry (AREA)
  • Developing Agents For Electrophotography (AREA)

Claims (30)

  1. Nichtmetallischer schwarzer Toner, der Tonerteilchen, die mindestens ein Bindemittelharz, einen Ruß und eine Organometallverbindung enthalten, und einen äußeren Zusatzstoff umfasst, wobei
    die Tonerteilchen 10 bis 200 ppm mindestens einer Art eines Alkalimetallelements enthalten;
    die Tonerteilchen mindestens eine Art einer Organometallverbindung enthalten, die aus Organoeisenverbindungen, Organoaluminiumverbindungen, Organochromverbindungen, Organozinkverbindungen, Organoborverbindungen und Organozirkoniumverbindungen ausgewählt ist;
    die Tonerteilchen als Harzbestandteil ein Polyesterharz enthalten und
    der nichtmetallische schwarze Toner
    einen massegemittelten Teilchendurchmesser von 4 bis 11 µm,
    die folgenden Verlusttangens tan δ, die durch das Verhältnis dielektrischer Verlustfaktor ε"/Dielektrizitätskonstante ε' bei Frequenzen von 5 × 104 Hz und 105 Hz gezeigt werden: tanδ  5 × 10 4  Hz ≤ 0 , 0125
    Figure imgb0035
     tanδ  10 5  Hz ≤ 0 , 0105 ,
    Figure imgb0036
    einen Carr-Fließfähigkeitsindex von 50 oder mehr und
    einen Carr-Flutbarkeitsindex von 65 oder mehr hat.
  2. Toner nach Anspruch 1, bei dem die Tonerteilchen 20 bis 170 ppm Alkalimetallelemente enthalten.
  3. Toner nach Anspruch 1, bei dem von den Alkalimetallelementen, die in den Tonerteilchen enthalten sind, meistens Kalium enthalten ist.
  4. Toner nach Anspruch 1, bei dem die Alkalimetallelemente in den Tonerteilchen in dem Ruß enthalten sind.
  5. Toner nach Anspruch 4, bei dem der Ruß 50 bis 1000 ppm Alkalimetallelemente, auf die Masse des Rußes bezogen, enthält.
  6. Toner nach Anspruch 1, bei dem die Organometallverbindung eine Organoeisenverbindung, eine Organoaluminiumverbindung oder eine Organozinkverbindung ist.
  7. Toner nach Anspruch 1, bei dem die Organometallverbindung eine Metallverbindung auf Azobasis ist.
  8. Toner nach Anspruch 1, bei dem die Organometallverbindung eine Hydroxycarbonsäure-Metallverbindung ist.
  9. Toner nach Anspruch 1, bei dem das Polyesterharz in den Tonerteilchen eine Säurezahl von 5 bis 30 mg KOH/g hat.
  10. Toner nach Anspruch 1, wobei der nichtmetallische schwarze Toner die folgenden Verlusttangens tan δ hat, die durch das Verhältnis dielektrischer Verlustfaktor ε"/Dielektrizitätskonstante ε' bei Frequenzen von 5 × 104 Hz und 105 Hz gezeigt werden: tanδ  5 × 10 4  Hz ≤ 0 , 0110
    Figure imgb0037
     tanδ  10 5  Hz ≤ 0 , 0090.
    Figure imgb0038
  11. Toner nach Anspruch 1, wobei der nichtmetallische schwarze Toner einen Carr-Fließfähigkeitsindex von 60 oder mehr und einen Carr-Flutbarkeitsindex von 75 oder mehr hat.
  12. Toner nach Anspruch 1, wobei der nichtmetallische schwarze Toner mit Wasser einen Kontaktwinkel von 110° oder mehr zeigt.
  13. Toner nach Anspruch 1, bei dem der Ruß einen mittleren Primärteilchendurchmesser von 13 bis 55 nm, einen pH-Wert von 7 oder mehr, einen Gehalt an flüchtigen Bestandteilen von 1 % oder weniger, eine DBP-Ölabsorption von 20 bis 100 ml für 100 g, einen Gehalt an mit Toluol extrahierbaren Bestandteilen von 0,1 % oder weniger, einen Siebrückstand von 250 ppm oder weniger und eine Schüttdichte von 650 g/Liter oder weniger hat.
  14. Toner nach Anspruch 13, bei dem der Ruß einen mittleren Primärteilchendurchmesser von 25 bis 50 nm hat.
  15. Toner nach Anspruch 13, bei dem der Ruß einen pH-Wert von 7,5 bis 10,5 hat.
  16. Toner nach Anspruch 13, bei dem der Ruß einen Gehalt an flüchtigen Bestandteilen von 0,8 % oder weniger hat.
  17. Toner nach Anspruch 13, bei dem der Ruß eine DBP-Ölabsorption von 30 bis 60 ml für 100 g hat.
  18. Toner nach Anspruch 13, bei dem der Ruß einen Gehalt an mit Toluol extrahierbaren Bestandteilen von 0,05 % oder weniger hat.
  19. Toner nach Anspruch 13, bei dem der Ruß einen Siebrückstand von 100 ppm oder weniger hat.
  20. Toner nach Anspruch 13, bei dem der Ruß eine Schüttdichte von 500 g/Liter oder weniger hat.
  21. Toner nach Anspruch 1, bei dem die Tonerteilchen 0,8 bis 20 Masseprozent des Rußes enthalten.
  22. Toner nach Anspruch 1, bei dem die Tonerteilchen 2 bis 15 Masseprozent des Rußes enthalten.
  23. Toner nach Anspruch 1, bei dem die Tonerteilchen 0,1 bis 8 Masseprozent der Organometallverbindung enthalten.
  24. Toner nach Anspruch 1, bei dem die Tonerteilchen 0,3 bis 6 Masseprozent der Organometallverbindung enthalten.
  25. Toner nach Anspruch 1, wobei der nichtmetallische schwarze Toner einen massegemittelten Teilchendurchmesser von 6 bis 9 µm hat.
  26. Toner nach Anspruch 1, wobei der Toner 20 Prozent (auf die Anzahl bezogen) oder weniger Teilchen mit einem Durchmesser von 4 µm oder weniger und 3,5 Volumenprozent oder weniger Teilchen mit einem Durchmesser von 12,7 µm oder mehr enthält.
  27. Bilderzeugungsverfahren mit
    einem Entwicklungsschritt, bei dem ein elektrostatisches Latentbild, das durch ein Latentbildträgerelement getragen wird, mit einem nichtmetallischen schwarzen Toner entwickelt wird und ein Tonerbild erzeugt wird;
    einem Übertragungsschritt, bei dem das auf dem Latentbildträgerelement erzeugte Tonerbild über ein Zwischenübertragungsmedium oder ohne Zwischenübertragungsmedium auf ein Aufzeichnungsmaterial übertragen wird; und
    einem Fixierschritt, bei dem das auf das Aufzeichnungsmaterial übertragene Tonerbild fixiert wird, wobei
    der nichtmetallische schwarze Toner nach einem der Ansprüche 1 bis 26 definiert ist.
  28. Bilderzeugungsverfahren nach Anspruch 27, bei dem das Tonerbild, das dem Fixierschritt zugeführt wird, ein Farbtonerbild ist, das den nichtmetallischen schwarzen Toner und einen farbigen Toner hat.
  29. Bilderzeugungsverfahren nach Anspruch 27, bei dem das Tonerbild, das dem Fixierschritt zugeführt wird, ein Vollfarben-Tonerbild ist, das den nichtmetallischen schwarzen Toner, einen cyanfarbenen (blaugrünen) Toner, einen magentafarbenen (purpurfarbenen) Toner und einen gelben Toner hat.
  30. Bilderzeugungsverfahren nach Anspruch 27, bei dem das Latentbildträgerelement ein elektrophotographisches lichtempfindliches Element ist.
EP00114307A 1999-07-05 2000-07-04 Toner und Bildherstellungsverfahren Expired - Lifetime EP1069479B1 (de)

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JP19006299 1999-07-05
JP19006299 1999-07-05
JP24474299 1999-08-31
JP24474299 1999-08-31
JP2000161883A JP3706790B2 (ja) 1999-07-05 2000-05-31 非磁性ブラックトナー及び画像形成方法
JP2000161883 2000-05-31

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EP1069479A1 EP1069479A1 (de) 2001-01-17
EP1069479B1 true EP1069479B1 (de) 2006-11-29

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JP6887833B2 (ja) 2016-03-18 2021-06-16 キヤノン株式会社 トナー及びトナーの製造方法
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JP7757029B2 (ja) 2020-03-24 2025-10-21 キヤノン株式会社 トナー
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EP1069479A1 (de) 2001-01-17
JP2001142258A (ja) 2001-05-25
US6316157B1 (en) 2001-11-13
JP3706790B2 (ja) 2005-10-19
DE60032066T2 (de) 2007-06-21

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